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Trimethyl orthoformate → HCID 9827593、化合物

HRID 351167
ノート
印刷プレビュー

反応式

HRID 351167 の反応式
C(OC([N:8]([CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=1)[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([CH2:16][NH:17][CH:18]2[C:27]3[N:26]=[CH:25][CH:24]=[CH:23][C:22]=3[CH2:21][CH2:20][CH2:19]2)=[CH:12][CH:11]=1)=O)(C)(C)C.C([N:42]1[CH2:46][CH2:45][C:44](=O)[CH2:43]1)(OC(C)(C)C)=O.COC(OC)OC.C([BH3-])#N.[Na+]>CO.C(O)(=O)C>[N:30]1[CH:31]=[CH:32][CH:33]=[CH:34][C:29]=1[CH2:28][NH:8][CH2:9][C:10]1[CH:11]=[CH:12][C:13]([CH2:16][N:17]([CH:44]2[CH2:45][CH2:46][NH:42][CH2:43]2)[CH:18]2[C:27]3[N:26]=[CH:25][CH:24]=[CH:23][C:22]=3[CH2:21][CH2:20][CH2:19]2)=[CH:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 9005Trimethyl orthoformateHCID 471360Tert-butyl 3-oxopyrrolidine-1-carboxylateHCID 5003444Sodium cyanoborohydrideHCID 22018600N-(t-butoxycarbonyl)-N-(2-pyridinylmethyl)-N'-(5,6,7,8-tetrahydro-8-quinolinyl)-1,4-benzenedimethanamine

生成物 1

HCID 9827593HCID 9827593、化合物収率 65.3%

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
触媒
HCID 887Methanol溶媒

実験手順

To the solution of N-(t-butyloxycarbonyl)-N-(2-pyridinylmethyl)-N′-(5,6,7,8-tetrahydro-8-quinolinyl)-1,4-benzenedimethanamine (195 mg, 0.43 mmol) and N-Boc-3-pyrrolidone (91 mg, 0.49 mmol) in methanol (3 ml) was added trimethylorthoformate (2 ml) and three drops of acetic acid, at room temperature. This mixture was allowed to stir for 30 min. at room temperature and sodium cyanoborohydride (130 mg, 2.09 mmol) was added. Stirring was continued for a further 18 hours at room temperature and then the reaction mixture was concentrated. The residue was dissolved in ethylacetate (300 mL), and washed with saturated aqueous NaHCO3 and brine, then dried (Na2SO4) and evaporated. Purification of the residue by column chromatography on silica gel (1.5×20 cm, 50:50 EtOAc/CH2Cl2) gave the desired product (120 mg, 45%) as a mixture of diastereomers.

後処理

  1. customat room temperature
  2. stirringStirring
  3. waitwas continued for a further 18 hours at room temperature
  4. concentrationthe reaction mixture was concentrated
  5. dissolutionThe residue was dissolved in ethylacetate (300 mL)
  6. washwashed with saturated aqueous NaHCO3 and brine
  7. dry with materialdried (Na2SO4)
  8. customevaporated
  9. customPurification of the residue by column chromatography on silica gel (1.5×20 cm, 50:50 EtOAc/CH2Cl2)

出典と根拠

ORDレコード
ord-3fcb0949974c4e2c923c159c3f6d7f0e
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07183273B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート